Uy, Alyssa V.

2BPh

Chapter 6: Powders and Granules  Pulverization by Intervention - Is the

reduction of particle size with the aid of a
Powders second agent which can be readily removed
 Pulvis from the pulverized product
 mixtures of finely divided drugs and/or chemicals used externally Ex.: applies to camphor where it
or internally in dry form is readily triturated when a few
 Advantages: drops of alcohol or other volatile
o More stable than liquid solvent is added. The pulverized
o More convenient to swallow than tablet or capsules camphor is readily recovered as
o Used in blending with medicated application as the solvent evaporates.
ointments, suppositories and pastes o Levigation - Is the process of reducing particle size by
o Can be prepared into granules for use in preparing first forming a paste of the solid with a minimum
tablets and or reconstituted to liquid form amount of a levigating agent and then triturating the
o Rapid therapeutic effect due to large surface area paste in a mortar or on slab with a spatula.
 Disadvantages:  The Basis of Choice of Levigating Agent is:
o Undesirability of taking bitter or unpleasant tasting of - Its ability to form a smooth
drugs paste with the substance
o Difficulty of protecting from decomposition those - Its compatibility in the product
powders containing hygroscopic, deliquescent or so water cannot be used for
aromatic materials levigating a substance for
o Time and expenses require in the preparation of oleaginous ointment base
uniform powders are great
Opening of Standard Sieves
o Inaccuracy of bulk powders
 Chemical & physical features
o morphology
o purity
o solubility
o Flowability
o stability
o particle size
o uniformity
o compatibility
 PRECAUTIONS IN PREPARING POWDERS TO BE OF HIGH EFFICACY
o The powders must be homogenous blend of all the
components  Medicated Powders
o Must be of the most advantageous particle size o Some medicated powders are intended to be used
internally; others externally
o Most powders for internal use are taken orally after
STEPS in PREPARING POWDERS
mixing with water
o Some powders are intended to be inhaled for local or
systemic effects
o @ Medicated powders for external use are dusted on
the affected area from sifter-type container or applied
from powder aerosol
o @ External use should bear a label marked EXTERNAL
USE ONLY
o Medicated for oral use may be intended for local
effects (laxatives) or systemic effect (analgesic)
 Aerosol Powders
o administered by inhalation with the aid of dry-powder
inhalers, which deliver micronized particles of
medication in metered quantities (range of 1 to 6 um)
 Particle Size Reduction o Ex.: Alupent; each dose is delivered through the
o Comminution or grinding may be defined as the mouthpiece upon activation of the aerosol unit’s valve
process of particle size reduction o it use in the treatment of asthma and other bronchial
METHODS OF COMMINUTION IN SMALL SCALE disorders
 Trituration - Is the process of grinding a  Particle Size Analysis (Powders of vegetable and animal drugs)
powder in a mortar and pestle to reduce its o Very coarse (No.8)
particle size. o Coarse (no. 20)
o Moderately coarse (No. 40)

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 o Fine (No. 60)
o Very Fine (No. 80)
o Coarse (No. 20)
o Moderately coarse (No. 40)
o Fine (No. 80)
o Very Fine (No. 120)
 Purpose: To obtain quantitative data on the size,
distribution, and shapes of drug and non drug
components to be used in pharmaceutical formulation
 Methods of determining particle size:
- SEDIMENTATION RATE, in which particles is
determined by measuring the terminal
settling velocity of particles through a liquid
medium in gravitational or centrifugal
environment (range: 0.8-300 micrometers)
- Light Energy diffraction, in which particle
size is determine by the reduction in light
reaching the sensor as the particle,
dispersed in a liquid or gas, passes through
the sensing zone (range: 0.2 - 500
micrometers)
- Laser halography, in which a pulsed laser is
fired through an aerolized particle spray
and photographed in three dimension with
a halographic camera, allowing the particles
to be individually imaged and sized (range:
1.4 - 100 micrometers)
- Cascade Impaction is based on the principle
that a particle, driven by an airstream, will
impact on a surface in its path, provided
that its inertia is sufficient to overcome the
drag force that tends to keep it in the
airstream
- SIEVING – particles are passed by
mechanical shaking through a series of
sieves (from 40 to 9500 micrometers,
depending upon sieve sizes)
- MICROSCOPY – particles are sized through
the use of calibrated grid background or
other measuring devise ( range 0.2 to 100
micrometers)
 Mixing powders
o Powders may be mixed or prepared depending upon
the nature of ingredients, the amount of powders to
be prepared, equipment available
o SPATULATION
 a method by which small amount of
powders may be blended by a spatula on a
sheet of paper or pill till.
 This is also applied to solid substances
which liquefy or form eutectic mixtures
Examples: phenol, camphor, menthol,
thymol, ASA, phenylsalicylate, and
phenacetin
o TRITURATION
 may be employed both to comminute and
to mix powder using mortar preferably with
a rough inner surface.
 In case a small amount of potent substance
is to be mixed with a large amount of
diluent, a general method known as
“geometric dilution” is employed to obtain
a uniform mix
o SIFTING
 the process of mixing by passing the
powder through sifters. Not generally
acceptable for potent drugs. Sifting results
in light puffy product.
o TUMBLING BY MECHANICAL MIXING
 the process of mixing powders by placing in
large containers or powder blenders the
rotates by tumbling motion
 Mixing by this process is thorough but time
consuming
o Dry Granulation
 Dry granulating, also called slugging or
roller compaction, involves the pressing of
mixed powders into an object to be
reground into a precise powder.
 This action increases particle density, and
improves powder flow.
o Milling
 Milling equipment is used to improve flow,
reduce segregation, enhance drying, and
limit wide particle size distribution
o Blending of Powders
 The "V" BLENDER is an efficient and
versatile blending machine for mixing and
lubrication process of dry powders
homogeneously
 The RIBBON BLENDER is an efficient and
versatile blending machine for mixing of dry
granules & powders homogeneously
 Packaging of Powders
o Bulk powders
1. Antacid or laxative powders, which the
patient generally takes by mixing the
directed amount of powder
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 2. Douche powder usually dissolved in warm
water by the patient for vaginal use
3. Dusting powders
4. Medicated or non medicated powders
5. Dentifrices or dental cleansing powders
6. Insufflations
7. Triturations
o DIVIDED POWDERS
 Latin - Chartulae, Abbr. “charts” or chartula
 After the powders have been properly
mixed by the geometric dilution, it may be
divided into individual units based upon the
dose. Method used is called “block and
divide”
 Powder papers:
2 3/4 x 3 3/4 inches,
3 x 4 1/2 inches,
3 3/4 x 5 inches and
4 1/2 x 6 inches
 SELECTION OF PAPER
 Hygroscopic or deliquescent - use water
proof or waxed paper
 Powders containing volatile components -
should be wrapped in waxed or in glassine
papers
 Powders containing neither volatile
components nor ingredients adversely
affected by air or moisture are usually be
wrapped in white papers
 Papers may be:
1. Simple bond papers
2. Vegetable parchment
3. Glassine, a glazed, transparent
paper
4. Waxed paper, a transparent
waterproof paper
 Ex. Of Finely Divided Powders:
1. Oral powders are supplied as
finely divided powders or as
effervescent granules
2. Douche powders, generally
dissolved in warm water for
vaginal use
3. Medicated or non medicated
powders for external application
usually dispensed in sifter cans
for convenient application to the
skin
4. Dentifrices or dental cleansing
powder
5. Denture powders, for dentifrices
or for adhesive to hold dentures
 Advantages Of Divided Powders
1. Flexibility
2. Rapid therapeutic effect
3. Stability
4. Ease of administration
 Disadvantages Of Divided Powders
1. Time consuming to prepare
2. Not well suited for dispensing of
many unpleasant tasting
hygroscopic drug
3. Inaccuracy
 Official Powdered Vegetable Drugs
1. Powdered Belladona Extract, NF
2. Powdered Digitalis Extract
3. Powdered Ipecac, USP
4. Powdered Opium, USP
5. Powdered Rauwolfia Serpentina,
NF
 Official Powders
1. Ampicillin Soluble Powder - dry
mixture of the ampicillin and
diluents and stabilising agents -
anti-infectives
2. Polymixin B Sulfate and
Bacitracin Zinc Topical Powder,
USP - used as a topical anti-
infective
3. Compound Clioquinol Powder,
USP - mixture of Clioquinol,
lactic acid, zinc stearate, and
lactose - vaginal insufflation as
an antitrichomonal
4. Nystatin Topical Powder, USP -
employed as a topical dusting
powder in the treatment of
mycotic infections
5. Tolnaftate Powder, USP - used
topically in the treatment of
fungal infection
 3 Official Powders For Topical Use:
1. Absorbable Dusting powder-
gloves lubricant
2. Compound
Iodochlorhydroxyquin Powder
NF - vaginal Insufflations as
antimicrobial
3. Methylbenzenethonium Choride
Powders NF - local anti-infectives
for diaper rash in infants
GRANULES
 are prepared agglomerates of smaller particles.
 They are generally irregularly shaped and behave as single larger
particles. They are usually in the 4 to 12 sieve size range
 Examples:
1. Pricipen (Ampicillin) for oral suspension (for
reconstitution)
2. Senokot Granules - for laxative
3. Effervescent products as Bromo Seltzer
4. K-lyte - Granulations of effervescent products-
compressed into tablet
 EFFERVESCENT GRANULATED SALTS
o Effervescent salts are granules or coarse to very coarse
powders containing a soluble medicinal agent in a dry
mixture
o Composition: Sodium bicarbonate, citric acid, and
tartaric acid
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o Note: When added to water, the acids and base react
to liberate CO2 resulting in effervescence
o Ex.: Sodium Phosphate - cathartic
o Reasons why effervescent salts are usually prepared
from a combination of citric acid and tartaric acid
rather than a single acid because of difficulties
presented as follows:
When tartaric acid is the sole acid, resulting granules
lose their firmness readily and crumble
Citric acid alone results in a sticky mixture difficult to
granulate
*So combination will give a balance and obtain a
satisfactory product.
o Method Of Preparation
1. Dry or Fusion method
2. Wet method
o Objectives Of Using The Methods
1. To determine the proper formula for the
preparation that will result in effective
effervescence and effect of the product
2. Efficient use of the acids and base present
3. Stable granulation
4. Pleasant taste
o Preparation of Granules
1. Dry Granulation
- the dry powder is passed through a roll
compactor and then through a
granulating machine
- a roll compactor, also called a roll press
or roller compactor, processes a fine
powder into dense sheets
- the surface of the compacting rolls may
be smooth or may have pocket
indentations or corrugations that allow
compaction of different forms and
textures
- the compacted powder is granulated to
uniform particle size in mechanical
granulator
- or dry method also termed slugging
2. Wet Granulation
Examples: Zantac EFFERdose tablets
o Lactinex Granules = mixed culture of
Lactobacillus acidophilus &Lactobacillus bulgaricus in 1
g packets used in the treatment of uncomplicated
diarrhea; mixed with water, beverages, sprinkled on
food, or eaten plain
o Official Effervescent Salt: Sodium Phosphate NF
Dried Sodium Phosphate (Dried and Powdered) 200 g
Sodium Bicarbonate (Dry Powder) 477 g
Tartaric acid (Dry Powder) 252 g
Citric acid, (Uneffluorescence crystals) 162 g
to make 1000 g
o A good working formula
Citric acid 15%
Tartaric acid 28%
Sodium bicarbonate 53%
o NOTE: Dose is assumed to be a heaping teaspoon (`5g).
Granules should be packaged in tight, dry wide mouth
glass jars in cool place
o Reactions:
1. H3C6H507.H20 + 3NaHCO3  Na3C6H5O7 + 4H2O + 3CO2
citric acid sodium citrate
2. H2C4H4O6 + 2NaHCO3  Na2C4H4O6 + 2H2O + 2CO2
tartaric acid
 It should be noted that it requires 3
molecules of NaHCO3 to neutralize 1
molecule of citric acid (1) and 2 molecules
of NaHCO3 to neutralize 1 molecule of
tartaric acid (2)
1. For the amount of NaHCO3 required to
neutralize 162 g citric acid:
162 g X (84 X 3 molecules)
210.13 252.03 MW NaHCO3
X = 194.3 g of NaHCO3
2. For the amount of NaHCO3 for neutralizing
252 g tartaric acid
252 g tartaric X (84 x2)
150.09 MW 168.02 g NaHCO3
X= 282.1 g NaHCO3
Total 194.3 + 282.1 = 476.4 g
o THE PROCEDURE: FUSION OR DRY METHOD
 Powder citric acid crystals
 Mix with other powders previously sieved
through #60 to ensure uniformity
 Place in a suitable dish in an oven
previously heated between 93-104oC
 During the heating, turn the powder with
an acid resistant spatula.
 It is removed from the oven and rubbed
through an acid resistant sieve to produce
granules of desired size
no. 4 sieve produce large granules
no. 8 sieve produced medium size granules
no. 10 sieve produced small granules
After sieving the granules are immediately
dried at a temperature not exceeding 54oC
the transfer immediately to a container &
promptly and tightly sealed.
o WET METHOD
 This differs from the fusion method in that
the source of binding agent is not
necessarily the water crystallization of citric
acid but may be water added to the
nonsolvent (such as alcohol) which is
employed as the moistening agent to form
the pliable mass of material for granulation.
 This granules may be compressed into
tablets form ( Bromo Seltzer by Warner
Lambert)
o DENTIFRICES
 Form of bulk powder, generally containing
flavors, soap or detergent, mild abrasive,
& an polishing agent.
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  Forms: paste, powder, liquid, and block or
solid
 Use: used with a tooth brush for the
purpose of cleansing the accessible
surfaces of the teeth.
 These contain abrasives such as Calcium
carbonate, calcium phosphate, calcium
sulfate, insoluble sodium metaphosphate,
hydrated Al2 O3 , MgCO3 and phosphates,
NaHCO3 and NaCl
 contain non-carbohydrates sweetening
agents but a few contain sugar
o Toothpaste
 contain liquids such as glycerin, propylene
glycol, sorbitol solution, water and
thickeners such as starch, tragacanth,
alginate and cellulose derivatives.
 Block form consist the following:
1. Polishing agents - calcium carbonate,
dibasic calcium phosphate dihydrate
or anhydrous, tricalcium phosphate,
calcium pyrophosphate, insoluble
sodium metaphosphate and hydrated
alumina
2. Massed with 20% to 30% of hard soap
and sufficient glycerol & flavoring oils
to retain an attractive appearance and
flavor
3. Tooth powders contain an abrasive, a
surface active detergent e.g. sodium
lauryl sulfate
4. Flavoring oils - spearmint,
peppermint, wintergreen, & cinnamon
mint
5. Sweetening agents - saccharin
6. Water
7. Humectant - glycerol, sorbitol,
propylene glycol
8. Binder - gums, karaya and tragacanth,
seaweed colloids: sodium alginate
&Irish moss extract, and synthetic
derivatives of cellulose:
methylcellulose and
carboxymethylcellulose
9. Preservatives - dichlorophene,
benzoates, and esters
10. Fluoride compounds - stannous and
sodium fluoride
 DOUCHE POWDERS
o Are products which are completely soluble and are
intended to be dissolved in water prior to use as
antiseptic or cleansing agent for a body cavity
o How to use: simply add the prescribed amount or
powder to the appropriate volume of warm water and
stirs until dissolved
o Components:
1. Boric acid or Borax
2. Astringents as K alum, ammonium alum,
ZnSO4
3. Antimicrobial as oxyquinoline sulfate or
povidone iodine
4. Quaternary ammonium compounds as
benzethonium chloride
5. Detergents as sodium lauryl sulfate
6. Oxidizing agents as sodium perborate
7. Salts, as sodium citrate, sodium chloride
8. Aromatic as menthol, thymol, eucalyptol,
methyl salicylate, and phenol
o Packaging: may be in a wide mouth glass jars to
protect from volatile constituents and by bulk powder
boxes
 DUSTING POWDERS
o Are non-toxic preparations for local application and
therefore no systemic effect.
o Dispensing: should be dispensed in a very fine
state of subdivision to enhance
effectiveness and minimized irritation
o Packaging: available in sifter-type containers or
pressure aerosols, the latter more
expensive but protects content from air,
moisture and contamination
o Uses: lubricants, absorbents, antiseptics,
antipruritics, astringents, & antiperspirant
 TRITURATIONS
o Are dilution of potent powdered drugs prepared by
intimately mixing them with a suitable diluents in a
definite proportion by weight. They were at one time
official as 1-10 dilutions.
o Preparation: in making trituration, geometric dilution is
used to assure thorough mixing. The active ingredient
is placed in a clean smooth, dry mortar. An equal bulk
(by estimation) of the weight diluents is added. It is
mixed quickly and twice as much diluents, not equal to
the amount in the mortar is added and mixed.
o Examples: Strychnine sulfate, arsenic, mercury
bichloride, atropine in convenient concentration using
lactose as the diluents for use at the Rx counter.
 INSUFFLATIONS
o Are finely divided powders introduced into the body
cavities such as the ears, nose, throat, tooth sockets
and vagina.
o Administration: Insufflator (powder blower) is usually
used, pressure aerosols are being employed especially
for potent drugs.
o Examples:
1. Norisodrine Sulfate Aerohaler
Cartridge (Abbott) - specialized
equipment or inhalation
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 2. Cromolyn Sodium Powder - relieve
bronchial asthma
 TEA
o Also known as “species” are made from coarsely
powdered dried herbs and are intended for use in
making medicinal teas and poultices

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